I.U. CINQUIMA, Analytical Chemistry Group, University of Valladolid, Valladolid, Spain.
J Sep Sci. 2013 Aug;36(16):2593-601. doi: 10.1002/jssc.201300310. Epub 2013 Jul 11.
A new and sensitive analytical method is presented to determine nine anticoagulant rodenticide (chlorophacinone, bromadiolone, pindone, diphacinone, warfarin, coumatetralyl, brodifacoum, floucomafen, and difenacoum) residues in water and soil samples by LC-ESI-MS. Rodenticides were extracted from soil using a methanol and ammonium formate 30 mM mixture, while ethyl acetate was employed in the water samples. A Gemini 5 μm C18 column was employed, and a mobile phase comprising a mixture of ammonium formate 30 mM and di-n-butylamine 30 mM in water (pH 3.5), ammonium formate 30 mM and di-n-butylamine 20 mM in water (pH 4.4), ammonium formate 30 mM in water (pH 6.5), and methanol in a gradient elution mode was selected. The method was fully validated and it was found to be selective and precise in terms of linearity and accuracy. Extraction recoveries ranged from 90 to 104% for the compounds studied, while the detection and quantification limits were between 0.09 and 2.2 μg/kg in soil or 0.08 and 1.7 μg/L in water. The method was applied to simultaneously measure these compounds in water and soil samples.
一种新的、灵敏的分析方法被提出,用于通过 LC-ESI-MS 测定水样和土壤样品中的九种抗凝杀鼠剂(氯杀鼠酮、溴敌隆、吡虫酮、敌鼠酮、华法林、氯鼠酮、溴鼠灵、氟鼠灵、杀鼠醚)残留。杀鼠剂从土壤中用甲醇和 30mM 甲酸铵混合物提取,而水样则采用乙酸乙酯提取。使用 Gemini 5μm C18 柱,选择包含 30mM 甲酸铵和 30mM 二正丁胺的水(pH3.5)、30mM 甲酸铵和 20mM 二正丁胺的水(pH4.4)、30mM 甲酸铵的水(pH6.5)和甲醇的梯度洗脱模式作为流动相。该方法经过全面验证,在线性和准确性方面具有选择性和精确性。对于所研究的化合物,提取回收率在 90%至 104%之间,而检测限和定量限在土壤中为 0.09 至 2.2μg/kg,在水中为 0.08 至 1.7μg/L。该方法被应用于同时测量水样和土壤样品中的这些化合物。